微波辅助酶解-超高效液相色谱串联质谱联用法快速检测尿液中的1-羟基芘

利用微波辅助酶解结合超高效液相色谱串联质谱联用法,建立了人体尿液中1-羟基芘的快速检测方法.通过对比酶解与碱解、恒温水浴酶解与微波辅助酶解、液液萃取与固相萃取等前处理方法对1-羟基芘检测的影响,最终采用微波辅助酶解、固相萃取作为样品检测的前处理方法.考察了基质效应,对比了纯溶剂与空白尿液配标准溶液2种不同的标准溶液配制方法,最终选用空白尿液来配制.方法的标准曲线方程为y=1.241 07x-0.130 042,相关系数为0.997 2,样品回收率在88.6%～97.1%之间,相对标准偏差在2.7%～12.6%之间,日内精密度为6.1%,日间精密度为6.2%,方法检测限为0.08 ng/mL,定量限为0.28 ng/mL.

Fast determination of 1 - hydroxypyrene in human urine by microwave assisted enzymatic hydrolysis-ultra performance liquid chromatography - tandem mass spectrometry

A method for fast determination of 1-hydroxypyrene (1-OHP) in human urinary by microwave assisted enzymatic hydrolysis-ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) was developed in this paper.The results of enzymatic hydrolysis compared with that of alkaline hydrolysis,microwave assisted enzymatic hydrolysis compared with that of water bath enzymatic hydrolysis,and the liquid-liquid extraction compared with that of solid phase extraction were discussed,respectively.The preparation of standard solutions by blank urine and pure solvent were studied to reduce the matrix effect. Finally,the microwave assisted enzymatic hydrolysis and solid phase extraction were selected and the blank urine was used to prepare the standard solutions.The standard curve equation of the method was y=1.241 07x-0.130 042.The correlation coefficient was 0.9972.The recovery was 88.6%—97.1%.The relative standard deviation was 2.7% to 12.6%.The intra-day precision was 6.1%.The inter-day precision was 6.2%.The detection limit was 0.08 ng /mL.The limit of quantification was 0.28 ng /mL.Compared with other existing methods,the established method in this paper for determination of urinary 1-hydroxypyrene was more simple and accurate.Its efficiency,reproducibility and sensitivity were also satisfying.